title: Development and validation method for the determination of selected tetracyclines in animal medicated feedingstuffs with the use of micellar liquid chromatography.
abstract: A chromatographic procedure for the determination of oxytetracycline (OTC), tetracycline (TC), chlorotetracycline (CTC), and doxycycline (DC) in medicated feedingstuffs was developed. Samples were extracted with 0.01 M citric buffer/acetonitrile (pH 3.0) and further purified with 0.45 μm syringe filters. The purified extract was separated on Thermo column C18, 150 × 4 mm, 5 μm and detection was carried out at 360 nm for OTC, and TC, 370 nm for CTC, and 350 nm for DC. TCs were eluted with a mobile phase of 0.03 M SDS/7% 1-butanol/0.02 M oxalic acid/NaOH at pH 2.5. This method provided average recoveries of 80.4% to 100.2%, with CVs of 0.5% to 6.6% in the range of 50 to 1500 mg/kg OTC, TC, CTC, and DC in feeds. The linearity for the four TCs was determined by high-performance liquid chromatography-diode array detector (HPLC-DAD) in the range 10-300 μg/mL (50-1500 mg/kg), with a linear correlation coefficient (R) > 0.99. The LOD and LOQ for TCs in pig and poultry feeds ranged from 4.0 to 10.7 and 4.7 to 12.6 mg/kg, respectively. The methodology was applied to the analysis of animal feedingstuffs collected from poultry and pig farms.
authors.affiliation: Department of Hygiene of Animal Feedingstuffs of National Veterinary Research Institute, Partyzantow 57, 24-100, Pulawy, Poland. ewelina.patyra@piwet.pulawy.pl
authors.forename: Ewelina
authors.initials: E
authors.lastname: Patyra
authors.forename: Ewelina
authors.initials: E
authors.lastname: Kowalczyk
authors.forename: Krzysztof
authors.initials: K
authors.lastname: Kwiatek
mesh_terms: D000465:Algorithms; D000821:Animal Feed / Q000032:analysis*; D000900:Anti-Bacterial Agents / Q000032:analysis; D002853:Chromatography, Liquid / Q000295:instrumentation* / Q000379:methods*; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D008823:Micelles; D013754:Tetracyclines / Q000032:analysis*
chemical_list: D000900:Anti-Bacterial Agents; D008823:Micelles; D013754:Tetracyclines